Flavoring composition



Patentedoct. 2a, 194;

- J Frederick J. Zimmerman and Wausau, Wia, uaignors to Maurice Earner, Salvo Chemical Corporation, Rothschild, Wis., a corporation of I Wisconsin No Drawing. Application January 25, 1945 Serial No. 574,628

'The present invention relates toan aqueous,

non-alcoholic, vanillin-containing flavoring composition,

Vanillin solutions have been extensively emplayed for flavoring purposes in place of extracts of vanilla. Vanilla contains about 2-3% of vanillin. Coumarin is frequently employedin conjunction with vanillin since their conjoint use produces an excellent vanilla-like flavor in foodstuffs ofvarious types. Thorough investigation demonstrates that, contrary to some authorities, vanillin is soluble only to the'extent of from 4-6 grams per liter in cold water (5-15 C.) and 6-8 grams per liter in water at room temperature. It has not been-possible, therefore, to produce an aqueous vanillin-containing flavoring composition 01 sufllcient potency to be commercially satisfactory since a concentration of grams per liter of vanillin is required as a practical minimum. As a result, it has been necessary to employ rather large percentages of aloholiup to 35% or more) and to prepare first an alcohol solution of vanillin followed by dilution of the alcohol solutionwith water. The general practice is' to dissolve 7-9 ounces of vanillin in 2.5 gallons of alcohol and to dilute the alcohol solution to about 10-12 gallons with water. Coumarin is less soluble in water than vanillin but since we employ only low concentrations of coumarin in our new vanillin composition we have no solubility problem in connection therewith.

Alcoholic vanillin extracts have, moreover, certain' recognized disadvantages, such as too rapid volatilization during baking or at raised temperatures, high cost, and a flavoring capacity less and somewhat diilerent than that desired or preferred, thus necessitating the use of increased amounts of the extracts, still further increasing the cost and often resulting in impaired or substandard product flavor. So far as we are aware, however, previous attempts to avoid these difliculties' by the use or vanillin have been unsuccessful since they usually resulted in the con-. version of the vanillin to sodium vanillin, which is practically valueless as a flavoring agent, or v have proceeded along other lines, such as the use of glycerine or other organic solvents and the deliberate formation of vanillin derivatives which have, however, not improved the situation.

In accordance with the present invention, aque-- ous vanillin-containing flavoring compositions are produced containing sufficient vanillin (and conmarin) to provide the desired flavor and flavor- Claims. (Cl. 99140) 5 to '7 by means of small additions of-an alkali of 6.6, and by adding small amounts of NaOH or ing power without using alcohol and without re-' sulting in the formation of substantial amounts or sodium vanillin or other undesirable or unhelpful vanillin derivatives. Since vanillin is an aidehyde (methylprotocatechuic aldehyde or 3-methoxy-4-hydroxy-benzaldehyde) it will be appreciated that it is comparatively reactive chemically and is relatively easily converted to sodiinnyanillin or to other derivatives. Our new flavoring composition is characterized also by the presence of small quantities or bufier salts which maintain the pH value of the composition between 5.0 and 7.0, under which conditions the solubility of vanillin is markedly increased so that without the use of alcohol it is possible to secure a potent flavoring composition suitable for general use in flavoring foodstuffs. This is surprising in view of the fact that it is generally known that vanillin is soluble in alkali hydroxide solutions in which, of

course, the pH is considerably greater than 7.0 a

and thus would lead to the expectation of poor solubility in neutral or acid solutions.

More specifically, our invention comprises a flavoring composition containing from about 10- j 15 grams per liter of vanillin and up to 2 grams per liter of coumarin plus a small amount of the sodium salt of a dibasic or tribasic acid. The pH value of the composition is adjusted to range from buffer salts we employ sodium phosphates, sodium citrate and sodium tartrate. NazHPQi is preferred. The buffer salts may be employed as such or may be formed in situ by the use of appropriate amounts of phosphoric acid, citric acid or tartaric acid with NaOH or equivalent.

The following examples illustrate our invention but do not limit it.

Example 1 r A stock solution was made up bydissolving 10 grams of vanillin and 0.1 gram of coumarin in 2.13 grams of Nazi-IP04 and adding suflicient water to. make one liter. This solution had a pH value citric acid the pH value could be adjusted anywhere 'within the range of 7-5, the addition oi. 0.4

gram of NaOH raising the pH value to 7.0 and the addition of 1.85 grams of citric acid lowering the pH value to 5.0. Lesser amounts of NaOH and citric acid yielded intermediate pH values.

that 6.3 grams per liter of Example 2 Example 3 A stock solution was made up in accordance with Example 1 but containing 8.52 grams of Nazi-IP04. The initial pH value was 7.25 which by means of citric acid additions ranging from 1.37 grams to 6.85 grams was lowered to 7.0-5.0

respectively, intermediate amounts of citric acid producing intermediate pH values.

While 0.1 gram per liter of coumarin has been set forth in the foregoing examples, we 'wish it to be understood that the coumarin concentration may be increased without departing from the invention and that up to 2 grams per liter of coumarin can be dissolved and successfully incorporatecl into our new compositions if desired, the precise amount employed depending upon the particular use to which the composition is to be put and the specific results desired. Generally We prefer a low coumarin concentration as set forth in the foregoing examples. While Nazi-IP04 is preferred and has been set forth in the examples, sodium citrate and sodium tartrate may also be satisfactorily employed as buffer saltsin molecularly proportionate amounts. The-compositions responding to our present invention are characterized by the fact that they are stable solutions and do not cause deposition of vanillin under refrigeration. Somewhat greater amounts .of vanillin than 10 grams per liter can be employed but we have found that 10 grams per-liter is adequate for practically allpurposes. vanillin concentrations up to approximately 15 grams per liter can be employed, however, and fall within and are deemed to be a part of our present invention. In using tartaric acid, we have found tartaric acid with 10 grams of vanillin and 0.1 gram of coumarin make a satisfactory flavoring composition, that a pH value of 5.0 is attained by adding 2.3 grams of NaOH per liter and that a pH value of 7.0 is attained by adding 3.0 grams of NaOH per liter. In using phosphoric acid, HIiPO i, we have found that 7.45 grams thereof may be employed with 10 grams of vanillin and 0.1 gram of coumarin per liter and that the pH range of 5.0 to 7.0 may be secured by adding 3.0 to 5.15 grams per liter, respectively, .of NaOI-I.

The buffer salts have the capacity to dissolve amounts of vanillin in excess of the amounts normally soluble in a given quantity of water and to prevent the deposition of the vanillin from such caramel or other brown coloring matter according to standard practices in preparing present vanillin extracts. We can, however, if we so desire, add a modicum of caramel or the like to our flavoring compositions without departing from the scope or spirit hereof.

The flavoring compositions are used in cookin baking and food-flavoring procedures in the same manner as alcoholic vanilla or vanillin extracts and therefore no alteration in standard processes is required by the use of our new flavoring composition. Within the scope of the appended claims, other and further additions, omissions, modifications and substitutions may be made without departing from the invention.

We claim:

1. An aqueous, non-alcoholic flavoring solution containing, per liter, about 10-15 grams of vanillin, about 0-2 grams! coumarin, at least one member of the group consisting of NBQIIPOIQ, NflZCdHAQG, NaaCsHaOv and reactants forming the same and the balance water, said solution being stable under refrigeration and having a permanent brown caramel-like color after standing.

2. An aqueous, non-alcoholic flavoring composition containing approximately 10 grams per liter 7 of vanillin, approximately 0.1 gram per liter of coumarin and suflicient NazI-IPOa to yield a pH value between 5 and 7.. and the balance water.

3. An aqueous flavoring solution containing the following ingredients in approximately the following relative amounts:

Vanillin rams per liter" 10-15 Coumarin do 0.12 Na HP0, dn 2.13-8.52

- A pH control agent Enough to produce a pH value between 5 and 7 Water Balance solution even under refrigeration for extended This characteristic makes it unnecessary to add In other words, the buffer salts.

4. An aqueous flavoring containing the following ingredients in approximately the following relative amounts:

Vanillin grams per liter Balance 5. An aqueous flavoring solution containing the following ingredients in approximately the following relative amounts:

vanillin rams per liter 10 Coumarm do 0.1 Na HP do 2.13 Water Balance 6. An aqueous fiavoring solution containingthe following ingredients in approximately the following relative amounts:

vanillin grams per liter 10 Coumarm d 0.1 Na HP04 do 4.26 Water Balance 7. An aqueous flavoring solution containing the following ingredients in approximately the following relative amounts:

Vanillin grams per liter 1O Coumarin fin 0.1 Na HP0 do 8.52 Citric acid do 1.37-6.85 Water Balance consisting of sodium phosphates, sodium citrate 5 and sodium tartrate sumcient to produce a pH value of 5-7.

9. A composition of matter containing vanillin and a small amount of one of the bufier salts enumerated in claim 8, said composition of matter being characterized by the capacity of dissolving in water to produce a stable, aqueous solution of a pH value of 5-7 in Whlch'the vanillin has a concentration of at least 10 grams per liter.

' FREDERICK J. ZIMMERMANN.

MAURICE KAYNER.

REFERENCES CITED The following references are of record in the file of this patent:

, 6 UNITED STATES PATENTS Number Name Date 1,515,714 Wussow Nov. 18, 1924 1,602,183 Thomssen Oct. 5, 19 2 6 5 2,033,612 Grifllth et a1 Mar. 3; i936 FOREIGN PATENTS I Number Country Date 490,646 Great Britain Aug. 18, 1938 OTHER REFERENCES Vanilla Extract, by Dean et al., The Journal of Industrial and Engineering Chemistry, July 1916, vol-8', No. 7, pages'60'1-614.

Certificate of Correction Patent No. 2,429,907 October 28, 1947 FREDERICK J. ZIMMERMANN ET AL. It is hereby certified that error appears in the printed specification of the above numbered patent requirmg correction as follows:

Column 4, line 38 after the word flavoring insert solution; line 58, for Na,HP, read make and that the said Letters Patent should be read as corrected above, so that the same may conform to the record of the case in the Patent Ofiice.

Signed and sealed this 19th day of December, A. D. 1950.

' THOMAS F. MURPHY,

Ann's tant Oommissioner of Paton. 

